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Ammonium Chloride → 3-(Trifluoromethoxy)pyridin-2-amine

HRID 2203652
Notes
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Reaction equation

HRID 2203652 reaction equation
[N+:1]([C:4]1[C:9]([O:10][C:11]([F:14])([F:13])[F:12])=[CH:8][CH:7]=[CH:6][N:5]=1)([O-])=O.[Cl-].[NH4+]>C(O)C.[Fe]>[F:14][C:11]([F:12])([F:13])[O:10][C:9]1[C:4]([NH2:1])=[N:5][CH:6]=[CH:7][CH:8]=1
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

5

Reactant 2

HCID 25517Ammonium ChlorideHCID 19034689HCID 19034689, compound

Product 1

HCID 498711863-(Trifluoromethoxy)pyridin-2-amine

Reagents, catalysts & solvents 2

HCID 23925IronCatalystHCID 702EthanolSolvent

Conditions

Temperature
70 °C

Procedure

To a stirred solution of 2-nitro-3-(trifluoromethoxy)pyridine (370 mg, 1.78 mmol) in ethanol (5 mL) were added aqueous ammonium chloride (951 mg, 17.78 mmol, in 10 mL of water) and iron powder (993 mg, 17.78 mmol). The reaction mixture was heated to 70° C. for 2 h. After cooling down the reaction mixture was filtered and the solid was washed with ethyl acetate. The mother liquid was concentrated to dryness in vacuo. The residue was diluted with water and extracted with ethyl acetate (3×15 mL). The combined organic layers were dried over anhydrous sodium sulfate and concentrated to dryness in vacuo. The residue was used in next step directly without further purification (250 mg, 79%): 1H NMR (400 MHz, DMSO-d6) δ 7.93-7.91 (m, 1H), 7.48-7.46 (m, 1H), 6.59-6.56 (m, 1H), 6.35 (brs, 2H).

Workup

  1. temperatureAfter cooling down the reaction mixture
  2. filtrationwas filtered
  3. washthe solid was washed with ethyl acetate
  4. concentrationThe mother liquid was concentrated to dryness in vacuo
  5. additionThe residue was diluted with water
  6. extractionextracted with ethyl acetate (3×15 mL)
  7. dry with materialThe combined organic layers were dried over anhydrous sodium sulfate
  8. concentrationconcentrated to dryness in vacuo
  9. customThe residue was used in next step directly without further purification (250 mg, 79%)

Sources & evidence

ORD record
ord-96f4d3aae38045bf9bb9b737d394ae85
Source dataset
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09365583B2

Reaction notes

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On this pageParticipantsConditionsProcedureWorkupSources & evidenceReaction notes